Process for making a detergent composition by non-tower process

ABSTRACT

A non-tower process for continuously preparing granular detergent composition having a density of at least about 600 g/l is provided. The process comprises the steps of (a) dispersing a surfactant and coating the surfactant with fine powder having a diameter from 0.1 to 500 microns in a mixer fitted with choppers, and (b) granulating the agglomerates in one or more fluidizing apparatus, wherein finely atomized liquid is sprayed onto the first agglomerates in a mixer between step (a) and (b).

FIELD OF THE INVENTION

The present invention generally relates to a non-tower process forproducing a particulate detergent composition. More particularly, theinvention is directed to a continuous process during which detergentagglomerates are produced by feeding a surfactant and coating materialsinto a series of mixers. The process produces a free flowing, detergentcomposition whose density can be adjusted for wide range of consumerneeds, and which can be commercially sold.

BACKGROUND OF THE INVENTION

Recently, there has been considerable interest within the detergentindustry for laundry detergents which are "compact" and therefore, havelow dosage volumes. To facilitate production of these so-called lowdosage detergents, many attempts have been made to produce high bulkdensity detergents, for example with a density of 600 g/l or higher. Thelow dosage detergents are currently in high demand as they conserveresources and can be sold in small packages which are more convenientfor consumers. However, the extent to which modern detergent productsneed to be "compact" in nature remains unsettled. In fact, manyconsumers, especially in developing countries, continue to prefer ahigher dosage levels in their respective laundering operations.

Generally, there are two primary types of processes by which detergentgranules or powders can be prepared. The first type of process involvesspray-drying an aqueous detergent slurry in a spray-drying tower toproduce highly porous detergent granules (e.g., tower process for lowdensity detergent compositions). In the second type of process, thevarious detergent components are dry mixed after which they areagglomerated with a binder such as a nonionic or anionic surfactant, toproduce high density detergent compositions (e.g., agglomeration processfor high density detergent compositions). In the above two processes,the important factors which govern the density of the resultingdetergent granules are the shape, porosity and particle sizedistribution of said granules, the density of the various startingmaterials, the shape of the various starting materials, and theirrespective chemical composition.

There have been many attempts in the art for providing processes whichincrease the density of detergent granules or powders. Particularattention has been given to densification of spray-dried granules bypost tower treatment. For example, one attempt involves a batch processin which spray-dried or granulated detergent powders containing sodiumtripolyphosphate and sodium sulfate are densified and spheronized in aMarumerizer®. This apparatus comprises a substantially horizontal,roughened, rotatable table positioned within and at the base of asubstantially vertical, smooth walled cylinder. This process, however,is essentially a batch process and is therefore less suitable for thelarge scale production of detergent powders. More recently, otherattempts have been made to provide continuous processes for increasingthe density of "post-tower" or spray dried detergent granules.Typically, such processes require a first apparatus which pulverizes orgrinds the granules and a second apparatus which increases the densityof the pulverized granules by agglomeration. While these processesachieve the desired increase in density by treating or densifying "posttower" or spray dried granules, they are limited in their ability to gohigher in surfactant active level without subsequent coating step. Inaddition, treating or densifying by "post tower" is not favourable interms of economics (high capital cost) and complexity of operation.Moreover, all of the aforementioned processes are directed primarily fordensifying or otherwise processing spray dried granules. Currently, therelative amounts and types of materials subjected to spray dryingprocesses in the production of detergent granules has been limited. Forexample, it has been difficult to attain high levels of surfactant inthe resulting detergent composition, a feature which facilitatesproduction of detergents in a more efficient manner. Thus, it would bedesirable to have a process by which detergent compositions can beproduced without having the limitations imposed by conventional spraydrying techniques.

To that end, the art is also replete with disclosures of processes whichentail agglomerating detergent compositions. For example, attempts havebeen made to agglomerate detergent builders by mixing zeolite and/orlayered silicates in a mixer to form free flowing agglomerates. Whilesuch attempts suggest that their process can be used to producedetergent agglomerates, they do not provide a mechanism by whichstarting detergent materials in the form of pastes, liquids and drymaterials can be effectively agglomerated into crisp, free flowingdetergent agglomerates.

Accordingly, there remains a need in the art to have an agglomeration(non-tower) process for continuously producing a detergent compositionhaving high density delivered directly from starting detergentingredients, and preferably the density can be achieved by adjusting theprocess condition. Also, there remains a need for such a process whichis more efficient, flexible and economical to facilitate large-scaleproduction of detergents (1) for flexibility in the ultimate density ofthe final composition, and (2) for flexibility in terms of incorporatingseveral different kinds of detergent ingredients, especially detergentingredients in the form of liquid, into the process.

The following references are directed to densifying spray-driedgranules: Appel et al, U.S. Pat. No. 5,133,924 (Lever); Bortolotti etal, U.S. Pat. No. 5,160,657 (Lever); Johnson et al, British patent No.1,517,713 (Unilever); and Curtis, European Patent Application 451,894.

The following references are directed to producing detergents byagglomeration: Beujean et al, Laid-open No. WO93/23,523 (Henkel), Lutzet al, U.S. Pat. No. 4,992,079 (FMC Corporation); Porasik et al, U.S.Pat. No. 4,427,417 (Korex); Beerse et al, U.S. Pat. No. 5,108,646(Procter & Gamble); Capeci et al, U.S. Pat. No. 5,366,652 (Procter &Gamble); Hollingsworth et al, European Patent Application 351,937(Unilever); Swatling et al, U.S. Pat. No. 5,205,958; Dhalewadikar et al,Laid Open No. WO96/04359 (Unilever).

For example, the Laid-open No. WO93/23,523 (Henkel) describes theprocess comprising pre-agglomeration by a low speed mixer and furtheragglomeration step by high speed mixer for obtaining high densitydetergent composition with less than 25 wt % of the granules having adiameter over 2 mm. The U.S. Pat. No. 4,427,417 (Korex) describescontinuous process for agglomeration which reduces caking and oversizedagglomerates.

None of the existing art provides all of the advantages and benefits ofthe present invention.

SUMMARY OF THE INVENTION

The present invention meets the aforementioned needs in the art byproviding a process which produces a high density granular detergentcomposition. The present invention also meets the aforementioned needsin the art by providing a process which produces a granular detergentcomposition for flexibility in the ultimate density of the finalcomposition from agglomeration (e.g., non-tower) process. The processdoes not use the conventional spray drying towers currently which islimited in producing high surfactant loading compositions. In addition,the process of the present invention is more efficient, economical andflexible with regard to the variety of detergent compositions which canbe produced in the process. Moreover, the process is more amenable toenvironmental concerns in that it does not use spray drying towers whichtypically emit particulates and volatile organic compounds into theatmosphere.

As used herein, the term "agglomerates" refers to particles formed byagglomerating raw materials with binder such as surfactants and orinorganic solutions/organic solvents and polymer solutions. As usedherein, the term "granulating" refers to fluidizing agglomeratesthoroughly for producing free flowing, round shapegranulated-agglomerates. As used herein, the term "mean residence time"refers to following definition:

mean residence time (hr)=mass (kg)/flow throughput (kg/hr)

All percentages used herein are expressed as "percent-by-weight" unlessindicated otherwise. All ratios are weight ratios unless indicatedotherwise. As used herein, "comprising" means that other steps and otheringredients which do not affect the result can be added. This termencompasses the terms "consisting of" and "consisting essentially of".

In accordance with one aspect of the invention, a process for preparinga granular detergent composition having a density at least about 600 g/lis provided.

The process comprises the steps of:

(a) dispersing a surfactant, and coating the surfactant with fine powderhaving a diameter from 0.1 to 500 microns, in a mixer wherein conditionsof the mixer include (i) from about 0.5 to about 15 minutes of meanresidence time and (ii) from about 0.15 to about 7 kj/kg of energycondition, wherein agglomerates are formed; and

(b) granulating the agglomerates in one or more fluidizing apparatuswherein conditions of each of the fluidizing apparatus include (i) fromabout 1 to about 10 minutes of mean residence time, (ii) from about 100to about 300 mm of depth of unfluidized bed, (iii) not more than about50 micron of droplet spray size, (iv) from about 175 to about 250 mm ofspray height, (v) from about 0.2 to about 1.4 m/s of fluidizing velocityand (vi) from about 12 to about 100° C. of bed temperature.

Also provided is a process for preparing a granular detergentcomposition having a density at least about 600 g/l, the processcomprises the steps of:

(a) dispersing a surfactant, and coating the surfactant with fine powderhaving a diameter from 0.1 to 500 microns, in a mixer wherein conditionsof the mixer include (i) from about 0.5 to about 15 minutes of meanresidence time and (ii) from about 0.15 to about 7 kj/kg of energycondition, wherein first agglomerates are formed;

(a') spraying finely atomized liquid onto the first agglomerates in amixer wherein conditions of the mixer include (i) from about 0.2 toabout 5 seconds of mean residence time, (ii) from about 10 to about 30m/s of tip speed, and (iii) from about 0.15 to about 5 kj/kg of energycondition, wherein second agglomerates are formed; and

(b) granulating the second agglomerates in one or more fluidizingapparatus wherein conditions of each of the fluidizing apparatus include(i) from about 1 to about 10 minutes of mean residence time, (ii) fromabout 100 to about 300 mm of depth of unfluidized bed, (iii) not morethan about 50 micron of droplet spray size, (iv) from about 175 to about250 mm of spray height, (v) from about 0.2 to about 1.4 m/s offluidizing velocity and (vi) from about 12 to about 100° C. of bedtemperature.

Also provided are the granular detergent compositions having a highdensity of at least about 600 g/l, produced by any one of the processembodiments described herein.

Accordingly, it is an object of the invention to provide a process forcontinuously producing a detergent composition which has flexibilitywith respect to density of the final products by controlling energyinput, residence time condition, and tip speed condition in the mixers.It is also an object of the invention to provide a process which is moreefficient, flexible and economical to facilitate large-scale production.These and other objects, features and attendant advantages of thepresent invention will become apparent to those skilled in the art froma reading of the following detailed description of the preferredembodiment and the appended claims.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

The present invention is directed to a process which produces freeflowing, granular detergent agglomerates having a density of at leastabout 600 g/l. The process produces granular detergent agglomerates froman aqueous and/or non-aqueous surfactant which is then coated with finepowder having a diameter from 0.1 to 500 microns, in order to obtain lowdensity granules.

Process

First Step (i) [Step(a)]

In the first step (i) of the process, one or more of aqueous and/ornon-aqueous surfactant(s) which is/are in the form of powder, pasteand/or liquid, and fine powder having a diameter from 0.1 to 500microns, preferably from about 1 to about 100 microns are fed into afirst mixer, so as to make agglomerates. (The definition of thesurfactants and the fine powder are described in detail hereinafter.)Optionally, an internal recycle stream of powder having a diameter ofabout 0.1 to about 300 microns generated in the fluidizing apparatus(e.g., fluid bed dryer and/or fluid bed cooler) can be fed into themixer in addition to the fine powder. The amount of such internalrecycle stream of powder can be 0 to about 60 wt % of final product.

Preferably, choppers which are attachable for the first mixer can beused to break up undesirable oversized agglomerates. Therefore, theprocess including the second with choppers is useful in order to obtainreduced amount of oversized agglomerates as final products, and suchprocess is one preferred embodiment of the present invention.

In another embodiment of the invention, the surfactant for the firststep (i) can be initially fed into a mixer or pre-mixer (e.g. aconventional screw extruder or other similar mixer) prior to the above,after which the mixed detergent materials are fed into the first mixeras described herein for agglomeration.

Generally speaking, preferably, the mean residence time of the firstmixer is in range from about 0.5 to about 15 minutes and the energy perunit mass of the first mixer (energy condition) is in range from about0.15 to about 7 kj/kg, more preferably, the mean residence time of thefirst mixer is from about 3 to about 6 minutes and the energy per unitmass of the first mixer (energy condition) is in range from about 0.15to about 4 kj/kg.

The examples of the first mixer can be any types of mixer known to theskilled in the art, as long as the mixer can maintain the abovementioned condition for the first step. An Example can be Lodige KMMixer manufactured by the Lodige company (Germany). As the result of thefirst step (i), the agglomerates (first agglomerates) are then obtained.The first agglomerates are then subjected to either (1) the second step,or (2) the first step (ii), followed by the second step.

First Step (ii) [Step (a')]

The resultant from the first step (i) (i.e., the first agglomerates) isfed into a second mixer. The first agglomerates are fed into a secondmixer, and then finely atomized liquid is sprayed on the agglomerates inthe second mixer. Optionally, excessive fine powder formed in the firststep (i) is added to the first step (ii). If the excessive fine powderis added to the first step (ii), spraying the finely atomized liquid isuseful in order to bind the excessive fine powder onto the surface ofagglomerates. About 0-10%, more preferably about 2-5% of powderdetergent ingredients of the kind used in the first step (i) and/orother detergent ingredients can be added to the second mixer.

Generally speaking, preferably, the mean residence time of the secondmixer is in range from about 0.2 to about 5 seconds and tip speed of themixer of the second mixer is in range from about 10 m/s to about 30 m/s,the energy per unit mass of the second mixer (energy condition) of thesecond mixer is in range from about 0.15 kj/kg to about 5 kj/kg, morepreferably, the mean residence time of the second mixer is in range fromabout 0.2 to about 5 seconds and tip speed of the second mixer is inrange from about 10 m/s to about 30 m/s, the energy per unit mass of thesecond mixer (energy condition) is in range from about 0.15 kj/kg toabout 5 kj/kg, the most preferably, the mean residence time of thesecond mixer is in range from about 0.2 to about 5 seconds, tip speed ofthe second mixer is in range from about 15 m/s to about 26 m/s, theenergy per unit mass of the second mixer (energy condition) is fromabout 0.2 kj/kg to about 3 kj/kg.

The examples of the second mixer can be any types of mixer known to theskilled in the art, as long as the mixer can maintain the abovementioned condition for the first step (ii). An Example can be FlexomicModel manufactured by the Schugi company (Netherlands). As the result ofthe first step (ii), the second agglomerates are then obtained.

Second Step [Step (b)]

In the second step, the first agglomerates from the first step (i), orthe second agglomerates from the first step (ii), are fed into afluidized apparatus, such as fluidized bed, in order to enhancegranulation for producing free flowing high density granules. The secondstep can proceed in one or more than one fluidized apparatus (e.g.,combining different kinds of fluidized apparatus such as fluid bed dryerand fluid bed cooler). Optionally, about 0 to about 10%, more preferablyabout 2-5% of powder detergent materials of the kind used in the firststep and/or other detergent ingredients can be added to the second step.Also, optionally, about 0 to about 20%, more preferably about 2 to about10% of liquid detergent materials of the kind used in the first step(i), the first step (ii) and/or other detergent ingredients can be addedto the step, for enhancing granulation and coating on the surface of thegranules.

Generally speaking, to achieve the density of at least about 600 g/l,preferably more than 650 g/l, condition of a fluidized apparatus can be;

Mean residence time: from about 1 to about 10 minutes

Depth of unfluidized bed: from about 100 to about 300 mm

Droplet spray size: not more than about 50 micron

Spray height: from about 175 to about 250 mm

Fluidizing velocity: from about 0.2 to about 1.4 m/s

Bed temperature: from about 12 to about 100° C.,

more preferably;

Mean residence time: from about 2 to about 6 minutes

Depth of unfluidized bed: from about 100 to about 250 mm

Droplet spray size: less than about 50 micron

Spray height: from about 175 to about 200 mm

Fluidizing velocity: from about 0.3 to about 1.0 m/s

Bed temperature: from about 12 to about 80° C.

If two different kinds of fluidized apparatus would be used, meanresidence time of the second step in total can be from about 2 to about20 minutes, more preferably, from about 2 to 12 minutes.

A coating agent to improve flowability and/or minimize overagglomeration of the detergent composition can be added in one or moreof the following locations of the instant process: (1) the coating agentcan be added directly after fluid bed cooler or fluid bed dryer; (2) thecoating agent may be added between fluid bed dryer and the fluid bedcooler; and/or (3) the coating agent may be added directly to fluid beddryer. The coating agent is preferably selected from the groupconsisting of aluminosilicates, silicates, carbonates and mixturesthereof. The coating agent not only enhances the free flowability of theresulting detergent composition which is desirable by consumers in thatit permits easy scooping for detergent during use, but also serves tocontrol agglomeration by preventing or minimizing over agglomeration. Asthose skilled in the art are well aware, over agglomeration can lead tovery undesirable flow properties and aesthetics of the final detergentproduct.

Starting Detergent Materials

The total amount of the surfactants in products made by the presentinvention, which are included in the following detergent materials,finely atomized liquid and adjunct detergent ingredients is generallyfrom about 5% to about 60%, more preferably from about 12% to about 40%,more preferably, from about 15 to about 35%, in percentage ranges. Thesurfactants which are included in the above can be from any part of theprocess of the present invention., e.g., from either one of the firststep (i), the first step (ii) and/or the second step of the presentinvention.

Detergent Surfactant (Aqueous/Non-aqueous)

The amount of the surfactant of the present process can be from about 5%to about 60%, more preferably from about 12% to about 40%, morepreferably, from about 15 to about 36%, in total amount of the finalproduct obtained by the process of the present invention.

The surfactant of the present process, which is used as the abovementioned starting detergent materials in the first step, is in the formof powdered, pasted or liquid raw materials.

The surfactant itself is preferably selected from anionic, nonionic,zwitterionic, ampholytic and cationic classes and compatible mixturesthereof. Detergent surfactants useful herein are described in U.S. Pat.No. 3,664,961, Norris, issued May 23, 1972, and in U.S. Pat. No.3,929,678, Laughlin et al., issued Dec. 30, 1975, both of which areincorporated herein by reference. Useful cationic surfactants alsoinclude those described in U.S. Pat. No. 4,222,905, Cockrell, issuedSep. 16, 1980, and in U.S. Pat. No. 4,239,659, Murphy, issued Dec. 16,1980, both of which are also incorporated herein by reference. Of thesurfactants, anionics and nonionics are preferred and anionics are mostpreferred.

Nonlimiting examples of the preferred anionic surfactants useful in thepresent invention include the conventional C₁₁ -C₁₈ alkyl benzenesulfonates ("LAS"), primary, branched-chain and random C₁₀ -C₂₀ alkylsulfates ("AS"), the C₁₀ -C₁₈ secondary (2,3) alkyl sulfates of theformula CH₃ (CH₂)_(x) (CHOSO₃ ⁻ M⁺) CH₃ and CH₃ (CH₂)_(y) (CHOSO₃ ⁻ M⁺)CH₂ CH₃ where x and (y+1) are integers of at least about 7, preferablyat least about 9, and M is a water-solubilizing cation, especiallysodium, unsaturated sulfates such as oleyl sulfate, and the C₁₀ -C₁₈alkyl alkoxy sulfates ("AE_(x) S"; especially EO 1-7 ethoxy sulfates).

Useful anionic surfactants also include water-soluble salts of2-acyloxy-alkane-1-sulfonic acids containing from about 2 to 9 carbonatoms in the acyl group and from about 9 to about 23 carbon atoms in thealkane moiety; water-soluble salts of olefin sulfonates containing fromabout 12 to 24 carbon atoms; and beta-alkyloxy alkane sulfonatescontaining from about 1 to 3 carbon atoms in the alkyl group and fromabout 8 to 20 carbon atoms in the alkane moiety.

Optionally, other exemplary surfactants useful in the paste of theinvention include C₁₀ -C₁₈ alkyl alkoxy carboxylates (especially the EO1-5 ethoxycarboxylates), the C₁₀₋₁₈ glycerol ethers, the C₁₀ -C₁₈ alkylpolyglycosides and the corresponding sulfated polyglycosides, and C₁₂-C₁₈ alpha-sulfonated fatty acid esters. If desired, the conventionalnonionic and amphoteric surfactants such as the C₁₂ -C₁₈ alkylethoxylates ("AE") including the so-called narrow peaked alkylethoxylates and C₆ -C₁₂ alkyl phenol alkoxylates (especially ethoxylatesand mixed ethoxy/propoxy), C₁₀ -C₁₈ amine oxides, and the like, can alsobe included in the overall compositions. The C₁₀ -C₁₈ N-alkylpolyhydroxy fatty acid amides can also be used. Typical examples includethe C₁₂ -C₁₈ N-methylglucamides. See WO 9,206,154. Other sugar-derivedsurfactants include the N-alkoxy polyhydroxy fatty acid amides, such asC₁₀ -C₁₈ N-(3-methoxypropyl) glucamide. The N-propyl through N-hexyl C₁₂-C₁₈ glucamides can be used for low sudsing. C₁₀ -C₂₀ conventional soapsmay also be used. If high sudsing is desired, the branched-chain C₁₀-C₁₆ soaps may be used. Mixtures of anionic and nonionic surfactants areespecially useful. Other conventional useful surfactants are listed instandard texts.

Cationic surfactants can also be used as a detergent surfactant hereinand suitable quaternary ammonium surfactants are selected from mono C₆-C₁₆, preferably C₆ -C₁₀ N-alkyl or alkenyl ammonium surfactants whereinremaining N positions are substituted by methyl, hydroxyethyl orhydroxypropyl groups. Ampholytic surfactants can also be used as adetergent surfactant herein, which include aliphatic derivatives ofheterocyclic secondary and tertiary amines; zwifterionic surfactantswhich include derivatives of aliphatic quaternary ammonium, phosphoniumand sulfonium compounds; water-soluble salts of esters ofalpha-sulfonated fatty acids; alkyl ether sulfates; water-soluble saltsof olefin sulfonates; beta-alkyloxy alkane sulfonates; betaines havingthe formula R(R¹)₂ N⁺ R² COO--, wherein R is a C₆ -C₁₈ hydrocarbylgroup, preferably a C₁₀ -C₁₆ alkyl group or C₁₀ -C₁₆ acylamido alkylgroup, each R¹ is typically C₁ -C₃ alkyl, preferably methyl and R₂ is aC₁ -C₅ hydrocarbyl group, preferably a C₁ -C₃ alkylene group, morepreferably a C₁ -C₂ alkylene group. Examples of suitable betainesinclude coconut acylamidopropyldimethyl betaine; hexadecyl dimethylbetaine; C₁₂₋₁₄ acylamidopropylbetaine; C₈₋₁₄ acylamidohexyldiethylbetaine; 4[C₁₄₋₁₆ acylmethylamidodiethylammonio]-1-carboxybutane; C₁₆₋₁₈acylamidodimethylbetaine; C₁₂₋₁₆ acylamidopentanediethylbetaine; and[C₁₂₋₁₆ acylmethylamidodimethylbetaine. Preferred betaines are C₁₂₋₁₈dimethyl-ammonio hexanoate and the C₁₀₋₁₈ acylamidopropane (or ethane)dimethyl (or diethyl) betaines; and the sultaines having the formula(R(R¹)₂ N⁺ R² SO₃ -- wherein R is a C₆ -C₁₈ hydrocarbyl group,preferably a C₁₀ -C₁₆ alkyl group, more preferably a C₁₂ -C₁₃ alkylgroup, each R¹ is typically C₁ -C₃ alkyl, preferably methyl, and R² is aC₁ -C₆ hydrocarbyl group, preferably a C₁ -C₃ alkylene or, preferably,hydroxyalkylene group. Examples of suitable sultaines include C₁₂ -C₁₄dimethylammonio-2-hydroxypropyl sulfonate, C₁₂ -C₁₄ amido propylammonio-2-hydroxypropyl sultaine, C₁₂ -C₁₄ dihydroxyethylammonio propanesulfonate, and C₁₆₋₁₈ dimethylammonio hexane sulfonate, with C₁₂₋₁₄amido propyl ammonio-2-hydroxypropyl sultaine being preferred.

Fine Powder

The amount of the fine powder of the present process, which is used inthe first step, can be from about 94% to 30%, preferably from 86% to54%, in total amount of starting material for the first step. Thestarting fine powder of the present process preferably selected from thegroup consisting of ground soda ash, powdered sodium tripolyphosphate(STPP), hydrated tripolyphosphate, ground sodium sulphates,aluminosilicates, crystalline layered silicates, nitrilotriacetates(NTA), phosphates, precipitated silicates, polymers, carbonates,citrates, powdered surfactants (such as powdered alkane sulfonic acids)and internal recycle stream of powder occurring from the process of thepresent invention, wherein the average diameter of the powder is from0.1 to 500 microns, preferably from 1 to 300 microns, more preferablyfrom 5 to 100 microns. In the case of using hydrated STPP as the finepowder of the present invention, STPP which is hydrated to a level ofnot less than 50% is preferable. The aluminosilicate ion exchangematerials used herein as a detergent builder preferably have both a highcalcium ion exchange capacity and a high exchange rate. Withoutintending to be limited by theory, it is believed that such high calciumion exchange rate and capacity are a function of several interrelatedfactors which derive from the method by which the aluminosilicate ionexchange material is produced. In that regard, the aluminosilicate ionexchange materials used herein are preferably produced in accordancewith Corkill et al, U.S. Pat. No. 4,605,509 (Procter & Gamble), thedisclosure of which is incorporated herein by reference.

Preferably, the aluminosilicate ion exchange material is in "sodium"form since the potassium and hydrogen forms of the instantaluminosilicate do not exhibit as high of an exchange rate and capacityas provided by the sodium form. Additionally, the aluminosilicate ionexchange material preferably is in over dried form so as to facilitateproduction of crisp detergent agglomerates as described herein. Thealuminosilicate ion exchange materials used herein preferably haveparticle size diameters which optimize their effectiveness as detergentbuilders. The term "particle size diameter" as used herein representsthe average particle size diameter of a given aluminosilicate ionexchange material as determined by conventional analytical techniques,such as microscopic determination and scanning electron microscope(SEM). The preferred particle size diameter of the aluminosilicate isfrom about 0.1 micron to about 10 microns, more preferably from about0.5 microns to about 9 microns. Most preferably, the particle sizediameter is from about 1 microns to about 8 microns.

Preferably, the aluminosilicate ion exchange material has the formula

    Na.sub.z [(AlO.sub.2).sub.z.(SiO.sub.2).sub.y ]xH.sub.2 O

wherein z and y are integers of at least 6, the molar ratio of z to y isfrom about 1 to about 5 and x is from about 10 to about 264. Morepreferably, the aluminosilicate has the formula

    Na.sub.12 [(AlO.sub.2).sub.12.(SiO.sub.2).sub.12 ]xH.sub.2 O

wherein x is from about 20 to about 30, preferably about 27. Thesepreferred aluminosilicates are available commercially, for example underdesignations Zeolite A, Zeolite B and Zeolite X. Alternatively,naturally-occurring or synthetically derived aluminosilicate ionexchange materials suitable for use herein can be made as described inKrummel et al, U.S. Pat. No. 3,985,669, the disclosure of which isincorporated herein by reference.

The aluminosilicates used herein are further characterized by their ionexchange capacity which is at least about 200 mg equivalent of CaCO₃hardness/gram, calculated on an anhydrous basis, and which is preferablyin a range from about 300 to 352 mg equivalent of CaCO₃ hardness/gram.Additionally, the instant aluminosilicate ion exchange materials arestill further characterized by their calcium ion exchange rate which isat least about 2 grains Ca⁺⁺ /gallon/minute/-gram/gallon, and morepreferably in a range from about 2 grains Ca⁺⁺/gallon/minute/-gram/gallon to about 6 grains Ca⁺⁺/gallon/minute/-gram/gallon.

Finely Atomized Liquid

The amount of the finely atomized liquid of the present process can befrom about 1% to about 10% (active basis), preferably from 2% to about6% (active basis) in total amount of the final product obtained by theprocess of the present invention. The finely atomized liquid of thepresent process can be selected from the group consisting of liquidsilicate, anionic or cationic surfactants which are in liquid form,aqueous or non-aqueous polymer solutions, water and mixtures thereof.Other optional examples for the finely atomized liquid of the presentinvention can be sodium carboxy methyl cellulose solution, polyethyleneglycol (PEG), and solutions of dimethylene triamine pentamethylphosphonic acid (DETMP).

The preferable examples of the anionic surfactant solutions which can beused as the finely atomized liquid in the present inventions are about88-97% active HLAS, about 30-50% active NaLAS, about 28% active AE3Ssolution, about 40-50% active liquid silicate, and so on.

Cationic surfactants can also be used as finely atomized liquid hereinand suitable quaternary ammonium surfactants are selected from mono C₆-C₁₆, preferably C₆ -C₁₀ N-alkyl or alkenyl ammonium surfactants whereinremaining N positions are substituted by methyl, hydroxyethyl orhydroxypropyl groups.

Preferable examples of the aqueous or non-aqueous polymer solutionswhich can be used as the finely atomized liquid in the presentinventions are modified polyamines which comprise a polyamine backbonecorresponding to the formula: ##STR1## having a modified polyamineformula V.sub.(n+1) W_(m) Y_(n) Z or a polyamine backbone correspondingto the formula: ##STR2## having a modified polyamine formulaV.sub.(n-k+1) W_(m) Y_(n) Y'_(k) Z, wherein k is less than or equal ton, said polyamine backbone prior to modification has a molecular weightgreater than about 200 daltons, wherein

i) V units are terminal units having the formula: ##STR3## ii) W unitsare backbone units having the formula: ##STR4## iii) Y units arebranching units having the formula: ##STR5## iv) Z units are terminalunits having the formula: ##STR6## wherein backbone linking R units areselected from the group consisting of C₂ -C₁₂ alkylene, C₄ -C₁₂alkenylene, C₃ -C₁₂ hydroxyalkylene, C₄ -C₁₂ dihydroxy-alkylene, C₈ -C₁₂dialkylarylene, --(R¹ O)_(x) R¹ --, --(R¹ O)_(x) R⁵ (OR¹)_(x) --, --(CH₂CH(OR²)CH₂ O)_(z) (R¹ O)_(y) R¹ (OCH₂ CH(OR²)CH₂)_(w) --, --C(O)(R⁴)_(r)C(O)--, --CH₂ CH(OR²)CH₂ --, and mixtures thereof; wherein R¹ is C₂ -C₆alkylene and mixtures thereof; R² is hydrogen, --(R¹ O)_(x) B, andmixtures thereof; R³ is C₁ -C₁₈ alkyl, C₇ -C₁₂ arylalkyl, C₇ -C₁₂ alkylsubstituted aryl, C₆ -C₁₂ aryl, and mixtures thereof; R⁴ is C₁ -C₁₂alkylene, C₄ -C₁₂ alkenylene, C₈ -C₁₂ arylalkylene, C₆ -C₁₀ arylene, andmixtures thereof; R⁵ is C₁ -C₁₂ alkylene, C₃ -C₁₂ hydroxyalkylene, C₄-C₁₂ dihydroxy-alkylene, C₈ -C₁₂ dialkylarylene, --C(O)--, --C(O)NHR⁶NHC(O)--, --R¹ (OR¹)--, --C(O)(R⁴)_(r) C(O)--, --CH₂ CH(OH)CH₂ --, --CH₂CH(OH)CH₂ O(R¹ O)_(y) R¹ OCH₂ CH(OH)CH₂ --, and mixtures thereof; R⁶ isC₂ -C₁₂ alkylene or C₆ -C₁₂ arylene; E units are selected from the groupconsisting of hydrogen, C₁ -C₂₂ alkyl, C₃ -C₂₂ alkenyl, C₇ -C₂₂arylalkyl, C₂ -C₂₂ hydroxyalkyl, --(CH₂)_(p) CO₂ M, --(CH₂)_(q) SO₃ M,--CH(CH₂ CO₂ M)CO₂ M, --(CH₂)_(p) PO₃ M, --(R¹ O)_(x) B, --C(O)R³, andmixtures thereof; oxide; B is hydrogen, C₁ -C₆ alkyl, --(CH₂)_(q) SO₃ M,--(CH₂)_(p) CO₂ M, --(CH₂)_(q) (CHSO₃ M)CH₂ SO₃ M, --(CH₂)_(q) --(CHSO₂M)CH₂ SO₃ M, --(CH₂)_(p) PO₃ M, --PO₃ M, and mixtures thereof; M ishydrogen or a water soluble cation in sufficient amount to satisfycharge balance; X is a water soluble anion; m has the value from 4 toabout 400; n has the value from 0 to about 200; p has the value from 1to 6, q has the value from 0 to 6; r has the value of 0 or 1; w has thevalue 0 or 1; x has the value from 1 to 100; y has the value from 0 to100; z has the value 0 or 1. One example of the most preferredpolyethyleneimines would be a polyethyleneimine having a molecularweight of 1800 which is further modified by ethoxylation to a degree ofapproximately 7 ethyleneoxy residues per nitrogen (PEI 1800, E7). It ispreferable for the above polymer solution to be pre-complex with anionicsurfactant such as NaLAS.

Other preferable examples of the aqueous or non-aqueous polymersolutions which can be used as the finely atomized liquid in the presentinvention are polymeric polycarboxylate dispersants which can beprepared by polymerizing or copolymerizing suitable unsaturatedmonomers, preferably in their acid form. Unsaturated monomeric acidsthat can be polymerized to form suitable polymeric polycarboxylatesinclude acrylic acid, maleic acid (or maleic anhydride), fumaric acid,itaconic acid, aconitic acid, mesaconic acid, citraconic acid andmethylenemalonic acid. The presence in the polymeric polycarboxylatesherein of monomeric segments, containing no carboxylate radicals such asvinylmethyl ether, styrene, ethylene, etc. is suitable provided thatsuch segments do not constitute more than about 40% by weight of thepolymer.

Homo-polymeric polycarboxylates which have molecular weights above 4000,such as described next are preferred. Particularly suitablehomo-polymeric. polycarboxylates can be derived from acrylic acid. Suchacrylic acid-based polymers which are useful herein are thewater-soluble salts of polymerized acrylic acid. The average molecularweight of such polymers in the acid form preferably ranges from above4,000 to 10,000, preferably from above 4,000 to 7,000, and mostpreferably from above 4,000 to 5,000. Water-soluble salts of suchacrylic acid polymers can include, for example, the alkali metal,ammonium and substituted ammonium salts.

Co-polymeric polycarboxylates such as a Acrylic/maleic-based copolymersmay also be used. Such materials include the water-soluble salts ofcopolymers of acrylic acid and maleic acid. The average molecular weightof such copolymers in the acid form preferably ranges from about 2,000to 100,000, more preferably from about 5,000 to 75,000, most preferablyfrom about 7,000 to 65,000. The ratio of acrylate to maleate segments insuch copolymers will generally range from about 30:1 to about 1:1, morepreferably from about 10:1 to 2:1. Water-soluble salts of such acrylicacid/maleic acid copolymers can include, for example, the alkali metal,ammonium and substituted ammonium salts. It is preferable for the abovepolymer solution to be pre-complexed with anionic surfactant such asLAS.

Adjunct Detergent Ingredients

The starting detergent material in the present process can includeadditional detergent ingredients and/or, any number of additionalingredients can be incorporated in the detergent composition duringsubsequent steps of the present process. These adjunct ingredientsinclude other detergency builders, bleaches, bleach activators, sudsboosters or suds suppressors, antitamish and anticorrosion agents, soilsuspending agents, soil release agents, germicides, pH adjusting agents,non-builder alkalinity sources, chelating agents, smectite clays,enzymes, enzyme-stabilizing agents and perfumes. See U.S. Pat. No.3,936,537, issued Feb. 3, 1976 to Baskerville, Jr. et al., incorporatedherein by reference.

Other builders can be generally selected from the various water-soluble,alkali metal, ammonium or substituted ammonium phosphates,polyphosphates, phosphonates, polyphosphonates, carbonates, borates,polyhydroxy sulfonates, polyacetates, carboxylates, andpolycarboxylates. Preferred are the alkali metal, especially sodium,salts of the above. Preferred for use herein are the phosphates,carbonates, C₁₀₋₁₈ fatty acids, polycarboxylates, and mixtures thereof.More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate,citrate, tartrate mono- and di-succinates, and mixtures thereof (seebelow).

In comparison with amorphous sodium silicates, crystalline layeredsodium silicates exhibit a clearly increased calcium and magnesium ionexchange capacity. In addition, the layered sodium silicates prefermagnesium ions over calcium ions, a feature necessary to insure thatsubstantially all of the "hardness" is removed from the wash water.These crystalline layered sodium silicates, however, are generally moreexpensive than amorphous silicates as well as other builders.Accordingly, in order to provide an economically feasible laundrydetergent, the proportion of crystalline layered sodium silicates usedmust be determined judiciously. Such crystalline layered sodiumsilicates are discussed in Corkill et al, U.S. Pat. No. 4,605,509,previously incorporated herein by reference.

Specific examples of inorganic phosphate builders are sodium andpotassium tripolyphosphate, pyrophosphate, polymeric metaphosphatehaving a degree of polymerization of from about 6 to 21, andorthophosphates. Examples of polyphosphonate builders are the sodium andpotassium salts of ethylene diphosphonic acid, the sodium and potassiumsalts of ethane 1-hydroxy-1, 1-diphosphonic acid and the sodium andpotassium salts of ethane, 1,1,2-triphosphonic acid. Other phosphorusbuilder compounds are disclosed in U.S. Pat. Nos. 3,159,581; 3,213,030;3,422,021; 3,422,137; 3,400,176 and 3,400,148, all of which areincorporated herein by reference.

Examples of nonphosphorus, inorganic builders are tetraboratedecahydrate and silicates having a weight ratio of SiO₂ to alkali metaloxide of from about 0.5 to about 4.0, preferably from about 1.0 to about2.4. Water-soluble, nonphosphorus organic builders useful herein includethe various alkali metal, ammonium and substituted ammoniumpolyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates.Examples of polyacetate and polycarboxylate builders are the sodium,potassium, lithium, ammonium and substituted ammonium salts of ethylenediamine tetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid,mellitic acid, benzene polycarboxylic acids, and citric acid.

Polymeric polycarboxylate builders are set forth in U.S. Pat. No.3,308,067, Diehl, issued Mar. 7, 1967, the disclosure of which isincorporated herein by reference. Such materials include thewater-soluble salts of homo- and copolymers of aliphatic carboxylicacids such as maleic acid, itaconic acid, mesaconic acid, fumaric acid,aconitic acid, citraconic acid and methylene malonic acid. Some of thesematerials are useful as the water-soluble anionic polymer as hereinafterdescribed, but only if in intimate admixture with the non-soap anionicsurfactant.

Other suitable polycarboxylates for use herein are the polyacetalcarboxylates described in U.S. Pat. No. 4,144,226, issued Mar. 13, 1979to Crutchfield et al, and U.S. Pat. No. 4,246,495, issued Mar. 27, 1979to Crutchfield et al, both of which are incorporated herein byreference. These polyacetal carboxylates can be prepared by bringingtogether under polymerization condition an ester of glyoxylic acid and apolymerization initiator. The resulting polyacetal carboxylate ester isthen attached to chemically stable end groups to stabilize thepolyacetal carboxylate against rapid depolymerization in alkalinesolution, converted to the corresponding salt, and added to a detergentcomposition. Particularly preferred polycarboxylate builders are theether carboxylate builder compositions comprising a combination oftartrate monosuccinate and tartrate disuccinate described in U.S. Pat.No. 4,663,071, Bush et al., issued May 5, 1987, the disclosure of whichis incorporated herein by reference.

Bleaching agents and activators are described in U.S. Pat. No.4,412,934, Chung et al., issued Nov. 1, 1983, and in U.S. Pat. No.4,483,781, Hartman, issued Nov. 20, 1984, both of which are incorporatedherein by reference. Chelating agents are also described in U.S. Pat.No. 4,663,071, Bush et al., from Column 17, line 54 through Column 18,line 68, incorporated herein by reference. Suds modifiers are alsooptional ingredients and are described in U.S. Pat. Nos. 3,933,672,issued Jan. 20, 1976 to Bartoletta et al., and 4,136,045, issued Jan.23, 1979 to Gault et al., both incorporated herein by reference.

Suitable smectite clays for use herein are described in U.S. Pat. No.4,762,645, Tucker et al, issued Aug. 9, 1988, Column 6, line 3 throughColumn 7, line 24, incorporated herein by reference. Suitable additionaldetergency builders for use herein are enumerated in the Baskervillepatent, Column 13, line 54 through Column 16, line 16, and in U.S. Pat.No. 4,663,071, Bush et al, issued May 5, 1987, both incorporated hereinby reference.

Optional Process Steps

Optionally, the process can comprise the step of spraying an additionalbinder in one or more than one of the first, second and/or the thirdmixers for the present invention. A binder is added for purposes ofenhancing agglomeration by providing a "binding" or "sticking" agent forthe detergent components. The binder is preferably selected from thegroup consisting of water, anionic surfactants, nonionic surfactants,liquid silicates, polyethylene glycol, polyvinyl pyrrolidonepolyacrylates, citric acid and mixtures thereof. Other suitable bindermaterials including those listed herein are described in Beerse et al,U.S. Pat. No. 5,108,646 (Procter & Gamble Co.), the disclosure of whichis incorporated herein by reference.

Other optional steps contemplated by the present process includescreening the oversized detergent agglomerates in a screening apparatuswhich can take a variety of forms including but not limited toconventional screens chosen for the desired particle size of thefinished detergent product. Other optional steps include conditioning ofthe detergent agglomerates by subjecting the agglomerates to additionaldrying by way of apparatus discussed previously.

Another optional step of the instant process entails finishing theresulting detergent agglomerates by a variety of processes includingspraying and/or admixing other conventional detergent ingredients. Forexample, the finishing step encompasses spraying perfumes, brightenersand enzymes onto the finished agglomerates to provide a more completedetergent composition. Such techniques and ingredients are well known inthe art.

Another optional step in the process involves surfactant pastestructuring process, e.g., hardening an aqueous anionic surfactant pasteby incorporating a paste-hardening material by using an extruder, priorto the process of the present invention. The details of the surfactantpaste structuring process are disclosed co-application No.PCT/US96/15960 (filed Oct. 4, 1996).

In order to make the present invention more readily understood,reference is made to the following examples, which are intended to beillustrative only and not intended to be limiting in scope.

EXAMPLES Example 1

The following is an example for obtaining agglomerates having highdensity, using Lodige KM mixer (KM-600), followed by Schugi FX-160Mixer, further followed by Fluid Bed Apparatus.

[Step 1] 120-260 kg/hr of HLAS (an acid precursor of C₁₁ -C₁₈ alkylbenzene sulfonate; 95% active) at about 45-60° C., is dispersed by thechoppers and/or the plows of KM-600 mixer along with 220 kg/hr ofpowdered STPP (mean particle size of 40-75 microns), 160-200 kg/hr ofground soda ash (mean particle size of 15 microns), 80-120 kg/hr ofground sodium sulfate (mean particle size of 15 microns), and 200 kg/hrof internal recycle stream of powder. Serrated plows can be used asmixing elements in the KM mixer. Choppers for the KM mixer can be usedto reduce the amount of oversized agglomerates. The condition of the KMmixer is as follows:

Mean residence time: 3-6 minutes

Energy condition: 0.15-2 kj/kg

Mixer speed: 100-150 rpm

Jacket temperature: 30-50° C.

[Step 2] The agglomerates from the KM-600 mixer are fed to the SchugiFX-160 mixer. 10-20 kg/hr of HLAS (an acid precursor of C₁₁ -C₁₈ alkylbenzene sulfonate; 94-97% active) is dispersed as finely atomized liquidin the Schugi mixer at about 50 to 60° C. 20-80 kg/hr of soda ash (meanparticle size of about 10-20 microns) is added in the Schugi mixer. Thecondition of the Schugi mixer is as follows:

Mean residence time: 0.2-5 seconds

Tip speed: 16-26 m/s

Energy condition: 0.15-2 kj/kg

Mixer speed: 2000-3200 rpm

[Step 3] The agglomerates from the Schugi mixer are fed to a fluid beddrying apparatus for drying, rounding and growth of agglomerates. 20-80kg/hr of liquid silicate (43% solids, 2.0 R) can be also added in thefluid bed drying apparatus at 35° C. The condition of the fluid beddrying apparatus is as follows:

Mean residence time: 4-8 minutes

Depth of unfluidized bed: 200 mm

Droplet spray size: less than 50 micron

Spray height: 175-250 mm (above distributor plate)

Fluidizing velocity: 0.4-0.8 m/s

Bed temperature: 40-70° C.]

The resultant from the step 3 has a density of about 700 g/l, and can besubjected to the optional process of cooling, sizing and/or grinding.

Example 2

The following is an example for obtaining agglomerates having highdensity, using Lodige KM mixer (KM-600), followed by Schugi FX-160Mixer, then Fluid Bed Apparatus.

[Step 1] 15 kg/hr-30 kg/hr of HLAS (an acid precursor of C₁₁ -C₁₈ alkylbenzene sulfonate; 95% active) at about 45-60° C. is dispersed by thechoppers and/or the plows of KM-600 mixer along with 220 kg/hr ofpowdered STPP (mean particle size of 40-75 microns), 160-200 kg/hr ofground soda ash (mean particle size of 15 microns), 80-120 kg/hr ofground sodium sulfate (mean particle size of 15 microns), and 200 kg/hrof internal recycle stream of powder. Serrated plows can be used asmixing elements in the KM mixer. Choppers for the KM mixer can be usedto reduce the amount of oversized agglomerates. The condition of the KMmixer is as follows:

Mean residence time: 3-6 minutes

Energy condition: 0.15-2 kj/kg

Mixer speed: 100-150 rpm

Jacket temperature: 30-50° C.

[Step 2] The agglomerates from the KM-600 mixer are fed to the SchugiFX-160 mixer. 10-25 kg/hr of neutralized AE₃ S liquid (25-28% active) isdispersed as finely atomized liquid in the Schugi mixer at about 30-40°C. 20-80 kg/hr of soda ash is added in the Schugi mixer. The conditionof the Schugi mixer is as follows:

Mean residence time: 0.2-5 seconds

Tip speed: 16-26 m/s

Energy condition: 0.15-2 kj/kg

Mixer speed: 2000-3200 rpm

[Step 3] The agglomerates from the Schugi mixer are fed to a fluid beddrying apparatus for drying, rounding and growth of agglomerates. 20-80kg/hr of liquid silicate (43% solids, 2.0 R) can be also added in thefluid bed drying apparatus at 35° C. The condition of the fluid beddrying apparatus is as follows:

Mean residence time: 2-4 minutes

Depth of unfluidized bed: 200 mm

Droplet spray size: less than 50 micron

Spray height: 175-250 mm (above distributor plate)

Fluidizing velocity: 0.4-0.8 m/s

Bed temperature: 40-70° C.]

The resultant from the step 3 has a density of about 700 g/l, and can besubjected to the optional process of cooling, sizing an/or grinding.

Example 3

The following is an example for obtaining agglomerates having highdensity, using Lodige KM mixer (KM-600), followed by Fluid Bed Apparatusfor further agglomerations.

[Step 1] 250-270 kg/hr of aqueous coconut fatty alcohol sulfatesurfactant paste (C₁₂ -C₁₈, 71.5% active), 40-80 kg/hr of HLAS (an acidprecursor of C₁₁ -C₁₈ alkyl benzene sulfonate; 94-97% active) is fed toa KM-600 mixer along with 220 kg/hr of powdered STPP (mean particle sizeof 40-75 microns), 160-200 kg/hr of ground soda ash (mean particle sizeof 15 microns), 80-120 kg/hr of ground sodium sulfate (mean particlesize of 15 microns), and 200 kg/hr of internal recycle stream of powder.The surfactant paste is fed at about 40 to 52° C., and the powders arefed at room temperature. Choppers for the KM mixer can be used to reducethe amount of oversized agglomerates. The condition of the KM mixer isas follows:

Mean residence time: 3-6 minutes

Energy condition: 0.15-2 kj/kg

Mixer speed: 100-150 rpm

Jacket temperature: 30-50° C.

[Step 2] The agglomerates from the KM mixer are fed to a fluid beddrying apparatus for drying, rounding and growth of agglomerates. 20-80kg/hr of liquid silicate (43% solids, 2.0 R) can be also added in thefluid bed drying apparatus at 35° C. The condition of the fluid beddrying apparatus is as follows:

Mean residence time: 2-4 minutes

Depth of unfluidized bed: 200 mm

Droplet spray size: less than 50 micron

Spray height: 175 -250 mm (above distributor plate)

Fluidizing velocity: 0.4-0.8 m/s

Bed temperature: 40-70° C.

The resultant from the step 3 has a density of at least 700 g/l, and canbe subjected to the optional process of cooling, sizing an/or grinding.

Having thus described the invention in detail, it will be obvious tothose skilled in the art that various changes may be made withoutdeparting from the scope of the invention and the invention is not to beconsidered limited to what is described in the specification.

What is claimed is:
 1. A non-tower process for preparing a granular detergent composition having a density of at least about 600 g/l, consisting of the steps of:(a) dispersing a surfactant, and coating the surfactant with fine powder having a diameter from 0.1 to 500 microns, in a mixer fitted with choppers wherein conditions of the mixer include (i) from about 0.5 to about 15 minutes of mean residence time and (ii) from about 0.15 to about 7 kj/kg of energy condition, wherein first agglomerates are formed; (a') spraying finely atomized liquid onto the first agglomerates in a mixer wherein conditions of the mixer include (i) from about 0.2 to about 5 seconds of mean residence time, (ii) from about 10 to about 30 m/s of tip speed, and (iii) from about 0.15 to about 5 kj/kg of energy condition, wherein second agglomerates are formed; (b) granulating the second agglomerates in one or more fluidizing apparatus wherein conditions of each of the fluidizing apparatus include (i) from about 1 to about 10 minutes of mean residence time, (ii) from about 100 to about 300 mm of depth of unfluidized bed, (iii) not more than about 50 micron of droplet spray size, (iv) from about 175 to about 250 mm of spray height, (v) from about 0.2 to about 1.4 m/s of fluidizing velocity and (vi) from about 12 to about 100° C. of bed temperature; (c) optionally dispersing an aqueous or non-aqueous polymer solution with said surfactant is step (a); (d) optionally adding an internal recycle stream of powder from the fluidizing apparatus to step (a); and (e) optionally adding excessive fine powder further formed in step (a) into step (a').
 2. The process according to claim 1 wherein said surfactant is selected from the group consisting of anionic surfactant, nonionic surfactant, cationic surfactant, zwitterionic, ampholytic and mixtures thereof.
 3. The process according to claim 1 wherein said surfactant is selected from the group consisting of alkyl benzene sulfonates, alkyl alkoxy sulfates, alkyl ethoxylates, alkyl sulfates, coconut fatty alcohol sulfates and mixtures thereof.
 4. The process according to claim 1 wherein the aqueous or non-aqueous polymer solution is dispersed with said surfactant in step (a).
 5. The process according to claim 1 wherein the fine powder is selected from the group consisting of soda ash, powdered sodium tripolyphosphate, hydrated tripolyphosphate, sodium sulphates, aluminosilicates, crystalline layered silicates, phosphates, precipitated silicates, polymers, carbonates, citrates, nitrilotriacetates, powdered surfactants and mixtures thereof.
 6. The process according to claim 1 wherein the internal recycle stream of powder from the fluidizing apparatus is added to step (a).
 7. The process according to claim 1 wherein the finely atomized liquid is selected from the group consisting of liquid silicates, anionic surfactants, cationic surfactants, aqueous polymer solutions, non-aqueous polymer solutions, water and mixtures thereof.
 8. The process according to claim 1 wherein the excessive fine powder is added to the step (a'). 